Hydrogen Bromide → HCID 22380865, compound

Participants

Reaction Steps

600 g of crude isoquinoline (purity 95% and total sulfur content 0.3%) and 759.6 g of 47% hydrobromic acid were stirred and cooled to undergo reaction. After the reaction, the resultant reactin mixture was distilled to expel water and then washed twice with acetone to afford 864.1 g of isoquinolinium bromide. By recrystallizing this isoquinolinium bromide from 6,881 g of isopropanol, 471.9 g (recovery ratio 85.9%) of refined isoquinolinium bromide having a total sulfur content of 22 ppm was obtained. The refined isoquinolinium bromide was recrystallized again from 6,498 g of isopropanol. The recrystallized isoquinolinium bromide (676.6 g) was dissolved in the same volume of water and decomposed with an aqueous 20% NaOH solution. Then, 495.3 g of the resultant liberated desulfurized isoquinoline was distilled, to afford 374.73 g (recovery ratio 62.5%) of refined isoquinoline (purity 99.7% and total sulfur content less than 1 ppm) was obtained.

Provenance & Evidence